Method for manufacturing a MXene nanodot composition using high pressure homogenization and a MXene nanodot composition manufactured by the method

Abstract

The present invention relates to a method for manufacturing a MXene nanodot composition using high-pressure homogenization and a MXene nanodot composition manufactured by the method. More specifically, the invention relates to a method for manufacturing MXene nanodots, characterized by generating nanoparticles by passing MXene through a spray module while pressurizing it to ultra-high pressure using a high-pressure homogenizer.

Description

Technology Field

[0001] The present invention relates to a method for preparing a MXene nanodot composition using high-pressure homogenization and a MXene nanodot composition prepared by the method. Background Technology

[0002] Homogenization is a process used to break down and mix materials to create a uniform and consistent mixture. It is commonly used in industries such as food, pharmaceuticals, and cosmetics to ensure a smooth texture, stability, and uniform distribution of ingredients.

[0003] A 'high-pressure homogenizer' is a machine that forcibly pushes liquid through small nozzles at very high pressure. This process reduces particle size, breaks down fat molecules, and improves the stability of emulsions or suspensions. It is widely used to improve texture and shelf life in milk processing, juice production, pharmaceutical formulations, and cosmetic creams.

[0004] Generally, high-pressure homogenizers utilize the principle of Bernoulli's theorem. When a fluid is pressurized to ultra-high pressure and passed through a spray module, shear, impact, and cavitation phenomena occur. This allows for the reduction of particles to a nano size of less than 1 µm. Since it can be used for purposes such as particle destruction, cell destruction, deagglomeration, dispersion, and fine emulsion accompanied by basic mixing processes, it is applicable in various research and industrial fields such as the chemical industry, food industry, pharmaceutical industry, cosmetic industry, and biotech. In particular, it is a device widely used to produce emulsions that serve as raw materials for cosmetics or inks, or to destroy the cell walls of cultured microorganisms.

[0005] A typical high-pressure homogenizer consists of a tank for storing fluid, a high-pressure pump for applying high pressure to the fluid flowing in from the tank, a spray module for passing the fluid through a spray channel under pressure from the high-pressure pump to cut it into nano-sizes and then emulsify it, and a heat exchanger for cooling the fluid that has passed through the spray module.

[0006] Figure 1 shows a configuration diagram of a conventional high-pressure homogenizer.

[0007] The operation of the high-pressure homogenizer configured as described above can be explained using the example of water and oil as follows. That is, a mixture of water and oil mixed by stirring is stored in a tank, and then the mixture of water and oil moves toward the injection module and passes through the injection channel of the injection module while receiving high pressure from a high-pressure pump. At this time, according to the Bernoulli principle described above, as the fluid mixed with water and oil passes through the very narrow injection channel at a very high speed, a shear force acts on the water and oil, causing them to break into nano-sized particles, thereby severing the connection structure of the aggregated molecules. After the fluid completely passes through the injection channel, the speed slows down in the wide passage, and the water and oil molecules that were broken are aggregated again by high pressure to produce an emulsion.

[0008] In the above-mentioned high-pressure homogenizer, a high-pressure pump is used to apply high pressure to the fluid, and a plunger pump is mainly used as the high-pressure pump.

[0009] Generally, a plunger pump used in a high-pressure homogenizer is configured such that a liquid end body and an isolator are screw-coupled, the outlet of a fluid storage tank is screw-coupled together with a ball-shaped valve to a fluid inlet port formed at the top of the liquid end bar, a plunger seal is inserted and installed in the seal mounting portion of the liquid end body, the plunger seal is secured by screw coupling with a seal retainer, and a plunger that reciprocates by a hydraulic cylinder is installed.

[0010] And as the above plunger reciprocates, the fluid flowing into the liquid and body is discharged through the outlet at high pressure.

[0011] In addition, MXene is a new nanomaterial with a two-dimensional structure that possesses high electrical conductivity and excellent solvent dispersibility (mainly in water and hydrophilic solvents), so research on the development of MXene and MXene / polymer composite materials is very active in fields such as flexible electrodes for printed electronics, thin-film sensors, high-power batteries and supercapacitors, and electromagnetic shielding.

[0012] MXenes are two-dimensional crystalline transition metal carbides, and 20 different MXene compositions have been synthesized so far, including Ti2C, Ti3C2, Nb2C, V2C, Ta4C3, Mo2TiC2, Mo2Ti2C3, and Cr2TiC2. These MXenes exhibit the best electrical conductivity among recently developed two-dimensional materials.

[0013] MXene can generally be synthesized from a ceramic material called MAX. MAX has a stacked structure of transition metals [e.g., titanium (Ti), niobium (Nb), vanadium (V), tantalum (Ta), molybdenum (Mo), chromium (Cr)], carbon, and group 14 elements [e.g., aluminum (Al) or silicon (Si), etc.], and a two-dimensional MXene is obtained by selectively removing only the group 14 elements through an etching process.

[0014] In almost all cases up to now, the above etching process has been carried out using strong acids in an aqueous medium, and as a result, terminal groups such as -OH, =O, -F, and -Cl are formed on the surface of MXene, and among them, particularly due to the -OH functional group, MXene has hydrophilic properties.

[0015] The MXene synthesized in this way possesses excellent water dispersion properties, and when formed into a film or sheet using processes such as filtering or bar coating, it achieves excellent electrical conductivity. Prior art literature

[0016] Republic of Korea Registered Patent No. 10-0898838 Republic of Korea Registered Patent No. 10-0806942 Republic of Korea Registered Patent No. 10-1937179 The problem to be solved

[0017] Accordingly, the present invention has been devised to solve the aforementioned conventional problems, and according to an embodiment of the present invention, the purpose is to provide a method for manufacturing a MXene nanodot composition using high-pressure homogenization, which can be applied by making MXene, a highly conductive material, into small dots of the OD shape, and a MXene nanodot composition manufactured by said method.

[0018] According to an embodiment of the present invention, the purpose is to provide a method for manufacturing a MXene nanodot composition using high-pressure homogenization, which is faster than the conventional hydrothermal method (manufacturing possible in seconds to minutes) and enables a continuous process by using a high-pressure homogenizer, and to provide a MXene nanodot composition manufactured by the same method, which can be applied by attaching drugs, fluorescent materials, etc. to functional groups such as -O, -OH.

[0019] Meanwhile, the technical problems to be solved by the present invention are not limited to those mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art to which the present invention belongs from the description below. means of solving the problem

[0020] The first objective of the present invention can be achieved as a method for manufacturing a MXene nanodot composition using high-pressure homogenization, characterized by generating nanoparticles by passing MXene through a spray module while pressurizing it to ultra-high pressure through a high-pressure homogenizer.

[0021] The second objective of the present invention can be achieved by a MXene nanodot composition characterized by being manufactured by the manufacturing method according to the first objective mentioned above.

[0022] And the two-dimensional MXene may be characterized by comprising at least one layer in which crystal cells having the empirical formula Mn+1Xn form a two-dimensional array, wherein X is located within an octahedral array formed by M, M is a metal selected from the group consisting of group IIIB metals, group IVB metals, group VB metals, and group VIB metals, X is C, N, or a combination thereof, and n=1, 2, 3, or 4.

[0023] In addition, the above two-dimensional MXene may be characterized by comprising at least one layer in which crystal cells having the empirical formula M'2M"nXn+1 form a two-dimensional array, wherein X is located within an octahedral array formed by M, M' and M" are different metals selected from the group consisting of group IIIB metals, group IVB metals, group VB metals, and group VIB metals, X is C, N, or a combination thereof, and n=1 or 2.

[0024] And it may be characterized by having a drug or fluorescent substance attached to the terminal functional group. Effects of the invention

[0025] According to the method for preparing a MXene nanodot composition using high-pressure homogenization according to an embodiment of the present invention and the MXene nanodot composition prepared by the method, the highly conductive material MXene can be made into small dots of the OD shape and applied.

[0026] According to the method for manufacturing a MXene nanodot composition using high-pressure homogenization according to an embodiment of the present invention and the MXene nanodot composition manufactured by the method, the top-down manufacturing method using a high-pressure homogenizer is faster than the conventional hydrothermal method (manufacturing is possible in seconds to minutes), a continuous process is possible, and the effect of attaching drugs, fluorescent substances, etc. to functional groups such as -O, -OH is applicable.

[0027] Meanwhile, the effects obtainable from the present invention are not limited to those mentioned above, and other unmentioned effects will be clearly understood by those skilled in the art to which the present invention belongs from the description below. Brief explanation of the drawing

[0028] The following drawings attached to this specification illustrate preferred embodiments of the present invention and serve to further enhance understanding of the technical concept of the present invention together with the detailed description of the invention; therefore, the present invention should not be interpreted as being limited only to the matters described in such drawings. FIG. 1 is a diagram of the configuration of a conventional high-pressure homogenizer, FIG. 2 is UV-vis spectroscopy according to an experimental example of the present invention, Figure 3 is a photograph of a MXene nanodot composition dispersed in a solvent according to an experimental example of the present invention, Figure 4 is an SEM image according to an experimental example of the present invention. Figure 5 shows an AFM according to an experimental example of the present invention. Specific details for implementing the invention

[0029] The above objects, other objects, features, and advantages of the present invention will be easily understood through the following preferred embodiments associated with the accompanying drawings. However, the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided to ensure that the disclosed content is thorough and complete, and to ensure that the spirit of the invention is sufficiently conveyed to a person skilled in the art.

[0030] In this specification, when a component is described as being on another component, it means that it may be formed directly on the other component or that a third component may be interposed between them. Also, in the drawings, the thicknesses of the components are exaggerated for the effective description of the technical content.

[0031] The embodiments described herein will be explained with reference to cross-sectional and / or plan views, which are exemplary illustrations of the invention. In the drawings, the thicknesses of films and regions are exaggerated for effective explanation of the technical content. Accordingly, the shapes of the exemplary drawings may be modified by manufacturing techniques and / or tolerances, etc. Accordingly, the embodiments of the invention are not limited to the specific shapes depicted but include variations in shape produced according to the manufacturing process. For example, a region depicted as a right angle may be rounded or have a certain curvature. Accordingly, the regions illustrated in the drawings have properties, and the shapes of the regions illustrated in the drawings are intended to illustrate specific shapes of the regions of the device and are not intended to limit the scope of the invention. Although terms such as first, second, etc., have been used to describe various components in the various embodiments of this specification, these components should not be limited by such terms. These terms are used merely to distinguish one component from another. The embodiments described and illustrated herein also include their complementary embodiments.

[0032] The terms used herein are for describing the embodiments and are not intended to limit the invention. In this specification, the singular form includes the plural form unless specifically stated otherwise in the text. As used herein, 'comprises' and / or 'comprising' do not exclude the presence or addition of one or more other components to the mentioned components.

[0033] In describing the specific embodiments below, various specific details have been included to explain the invention more specifically and to aid understanding. However, a reader with sufficient knowledge in the art to understand the invention will recognize that it can be used without these various specific details. In some cases, it is noted in advance that commonly known aspects that are not significantly related to the invention have been omitted to prevent unnecessary confusion in describing the invention.

[0035] Hereinafter, a method for preparing a MXene nanodot composition using high-pressure homogenization according to an embodiment of the present invention, and a MXene nanodot composition characterized by being prepared by said method will be described.

[0036] A method for preparing a MXene nanodot composition using high-pressure homogenization according to an embodiment of the present invention prepares a MXene nanodot composition by pressurizing MXene to ultra-high pressure through a high-pressure homogenizer and passing it through a spray module to generate nanoparticles.

[0037] According to an embodiment of the present invention, MXene, a highly conductive material, can be made into small dots of the OD shape and applied.

[0038] According to an embodiment of the present invention, a top-down manufacturing method using a high-pressure homogenizer allows for faster processing (manufacturing possible in seconds to minutes) and a continuous process compared to the conventional hydrothermal method.

[0039] In addition, drugs, fluorescent materials, etc., can be attached to functional groups such as -O and -OH of the MXene nanodot composition for application.

[0040] 2D MXene is M n+1 X nThe structure comprises at least one layer in which crystal cells having the empirical formula are arranged in a two-dimensional array, wherein X is located within an octahedral array formed by M. M is a metal selected from the group consisting of group IIIB metals, group IVB metals, group VB metals, and group VIB metals, X is C, N, or a combination thereof, and n=1, 2, 3, or 4.

[0041] Also, two-dimensional MXenes are M'2M" n X n+1 The structure comprises at least one layer in which crystal cells having the empirical formula are arranged in a two-dimensional array, wherein X is located within an octahedral array formed by M. M' and M" are different metals selected from the group consisting of group IIIB metals, group IVB metals, group VB metals, and group VIB metals, X is C, N, or a combination thereof, and n=1 or 2.

[0042] In one embodiment, M may be, for example, Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, or a combination thereof, but is not limited thereto, and M n+1 The empirical formula of Xn may be, for example, Sc2C, Ti2C, Ti3C2, Nb2C, V2C, Ta4C3, Mo2TiC2, Mo2Ti2C3, Cr2TiC2, Ti2N, Ti3CN, Mo2C, Nb4C3, Zr3C2, Ti4N3, V4C3, Hf3C2, Mo2N, Cr2C, Zr2C, Nb2C, Hf2C, V3C2, Ta3C2, or Ti4C3, but is not limited thereto.

[0043] In another embodiment, the two-dimensional MXene may include at least one layer in which crystal cells having the empirical formula M'2M"nXn+1 form a two-dimensional array.

[0044] Here, each X is located within an octahedral array consisting of multiple M' and M", where M' and M" are different metals selected from the group consisting of group IIIB metals, group IVB metals, group VB metals and group VIB metals, each X is C, N or a combination thereof, and n can be 1 or 2.

[0045] In other embodiments, M may be, for example, Ti, V, Nb, Ta, Cr, Mo, or a combination thereof, but is not limited thereto, and M'2M" n X n+1 The empirical formula of may be, for example, Mo2VC2, Mo2TaC2, Mo2NbC2, Cr2VC2, Cr2TaC2, Cr2NbC2, Ti2TaC2, Ti2NbC2, V2TaC2, V2TiC2, Mo2V2C3, Mo2Nb2C3, Mo2Ta2C3, Cr2Ti2C3, Cr2Ta2C3, Cr2V2C3, Cr2Nb2C3, Nb2Ta2C3, Ti2Nb2C3, Ti2Ta2C3, V2Nb2C3, V2Ta2C3, or V2Ti2C3.

[0046] Two-dimensional MXenes may be free-standing two-dimensional assemblies in which the crystal structures are independent and continuous, or stacked assemblies in which the crystal structures are stacked. In the case of stacked assemblies, atoms, ions, or molecules may be interlayer-inserted between at least a few layers, and the atoms or ions interlayer-inserted may be lithium. Accordingly, the surface-modified two-dimensional MXene according to one embodiment of the present invention may also be used in energy storage devices such as batteries and supercapacitors.

[0047] In addition, the two-dimensional MXene particles surface-modified with phosphates containing saturated or unsaturated hydrocarbons according to the present invention can retain excellent electrical conductivity, magnetic loss, and dielectric loss characteristics, which are inherent characteristics of the two-dimensional MXene particles themselves before surface modification, and thus can be used as conductive flexible electrodes, heaters, or electromagnetic wave absorbers.

[0048] MXene can be synthesized by etching the MAX phase.

[0049] Non-limiting examples of etching agents for etching the MAX phase to produce MXene include strong etching agents containing F, such as HF, NH4HF2, and a mixture of HCl and LiF. For example, when Ti3AlC2 is etched in an aqueous HF solution at room temperature, Al atoms are selectively removed, and O, OH, and F atoms are formed as terminal functional groups on the carbide layers.

[0050] Accordingly, the MXenes produced by etching in the present invention can be represented as Mn+1Xn(Tx) or M'2M"nXn+1(Tx), where Tx represents terminal groups such as -OH,=O, and -F formed through etching.

[0052] Hereinafter, experimental examples and experimental result data according to the embodiments of the present invention mentioned above will be described.

[0053] In the experimental example of the present invention, the pressure of the high-pressure homogenizer is 400 to 2,000 bar, and the repeat times are 1 to 4 times (2 times: 2P, 3 times: 3P, 4 times: 4P).

[0054] Multi-Layered MXene (ML-MXene) was applied as the material, and the operating pressure of the equipment and the number of times the ML-MXene passed through the equipment were controlled.

[0055] Figure 2 shows UV-vis spectroscopy according to an experimental example of the present invention.

[0056] As shown in Figure 2, all three samples exhibit a graph shape similar to that of Mxene. However, they display an oxidized form in which the Ti-O (250 nm) peak is larger than the Ti-C (320 nm) peak. This shape indicates that the size of the Ti-O peak increases with each passing through HPH, suggesting further oxidation. By controlling the degree of oxidation, the generation of TiO2 can be controlled for various applications (catalytic applications are possible).

[0057] Figure 3 shows a photograph of a MXene nanodot composition dispersed in a solvent according to an experimental example of the present invention. As shown in Figure 3, it can be seen that the Tyndall effect occurs due to very high dispersibility.

[0058] Figure 4 shows an SEM image according to an experimental example of the present invention. As shown in Figure 4, it can be seen that the film produced by filtering has a structure in which small-sized MXene nanoparticles are aggregated.

[0059] Figure 5 shows an AFM according to an experimental example of the present invention. As shown in Figure 5, it can be seen that a nanodot shape with a thickness of 2 nm and a width of several hundred nanometers is observed.

[0061] In addition, the device and method described above are not limited to the configurations and methods of the embodiments described above; rather, all or part of each embodiment may be selectively combined to allow for various modifications to be made.

Claims

Claim 1 A method for manufacturing a MXene nanodot composition using high-pressure homogenization, characterized by generating nanoparticles by passing MXene through a spray module while pressurizing it to ultra-high pressure through a high-pressure homogenizer. Claim 2 A MXene nanodot composition characterized by being manufactured by the manufacturing method according to claim 1. Claim 3 A MXene nanodot composition according to claim 2, wherein the two-dimensional MXene comprises at least one layer in which crystal cells having the empirical formula Mn+1Xn form a two-dimensional array, wherein X is located within an octahedral array formed by M, wherein M is a metal selected from the group consisting of group IIIB metals, group IVB metals, group VB metals, and group VIB metals, and X is C, N, or a combination thereof, and n=1, 2, 3, or 4. Claim 4 A MXene nanodot composition according to claim 3, wherein the two-dimensional MXene comprises at least one layer in which crystal cells having the empirical formula M'2M"nXn+1 form a two-dimensional array, wherein X is located within an octahedral array formed by M, M' and M" are different metals selected from the group consisting of group IIIB metals, group IVB metals, group VB metals, and group VIB metals, and X is C, N, or a combination thereof, and n=1 or 2. Claim 5 A MXene nanodot composition characterized by having a drug or fluorescent substance attached to a terminal functional group in claim 4.

Images